CN106543732A - A kind of diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method - Google Patents
A kind of diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method Download PDFInfo
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- CN106543732A CN106543732A CN201610916971.XA CN201610916971A CN106543732A CN 106543732 A CN106543732 A CN 106543732A CN 201610916971 A CN201610916971 A CN 201610916971A CN 106543732 A CN106543732 A CN 106543732A
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- type silsesquioxane
- cage
- diphenyl siloxy
- heat
- silicon rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
- C08L2312/08—Crosslinking by silane
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A kind of diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method, it is related to a kind of silicone rubber preparation method, there is additive reaction at room temperature in vinyl of the cage-type silsesquioxane containing si-h bond of the invention in the presence of catalyst and in silicone rubber, while cage-type silsesquioxane inorganic skeleton and benzene ring structure are introduced in silicone rubber.By methyl phenyl vinyl silicone oil, diphenyl siloxy cage-type silsesquioxane cross-linking agent, metal-oxide, PC610 catalyst-initiators, under Pt catalyst actions, there is additive reaction in cage-type silsesquioxane and silicone rubber medium vinyl, prepare novel Room Temperature sulphurated siliastic, the present invention can be used at a temperature of 460 DEG C for a long time, and compared with original silicone rubber, thermostability is more preferably, easy to use.
Description
Technical field
The present invention relates to a kind of silicone rubber preparation method, more particularly to a kind of diphenyl siloxy cage-type silsesquioxane
Heat-resistant silicon rubber preparation method.
Background technology
Silicone rubber is a kind of with excellent thermostability, insulating properties, antidetonation, measuring body specific rubber, and room temperature vulcanization
Silicone rubber is easy to use, without the need for hot setting, is with a wide range of applications, and common silicon rubber heat-resisting is at 200 DEG C -300 DEG C
Between, but with the continuous development of science and technology, especially Aero-Space and high ferro technical requirements silicone rubber are higher
At a temperature of life-time service, therefore further improve silicone rubber thermostability make great sense.Chinese patent
CN102643553A discloses a kind of high-temperature-resisting silicon rubber additive and method, and heat-resisting additive prepared by the method can make
The heat resisting temperature of silicone rubber reaches 300 DEG C, it is impossible to meet the heat resistant requirements to silicone rubber under specific condition；Chinese patent
CN103087532A discloses a kind of Addition-type heat-resistant silicon rubber and preparation method thereof, silicon rubber heat-resisting temperature prepared by the method
Reach 460 DEG C, although in temperature, can reach application requirement, but the auxiliary packing added in formula is more, considerably beyond
The number of matrix material, although heat resisting temperature is higher, but the compatibility is poor, mechanical property can be affected, it is impossible to reach
Application requirement.
The content of the invention
It is an object of the invention to provide a kind of diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method,
I.e. vinyl of the cage-type silsesquioxane containing si-h bond in the presence of catalyst and in silicone rubber occurs to add at room temperature
Into reaction, while cage-type silsesquioxane inorganic skeleton and benzene ring structure are introduced in silicone rubber.The present invention can be at 460 DEG C
At a temperature of use for a long time, compared with original silicone rubber, thermostability is more preferably, easy to use.
The purpose of the present invention is achieved through the following technical solutions：
A kind of diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method, methods described include that following preparation walks
Suddenly：
i）The synthesis of diphenyl siloxy cage-type silsesquioxane；
ii）Methyl phenyl vinyl silicone oil is sequentially added, metal-oxide, PC610 inhibitor, Pt platinum catalysts, machinery are stirred
Mix mix homogeneously, 100 DEG C of vaccum dewatering 5h；Add the diphenyl siloxy cage model sesquialter silicon for being dissolved in hexamethylene of above-mentioned preparation
Oxygen alkane cross-linking agent, the bubble after mix homogeneously in low pressure removing system can be fully cured after heat treatment 4h at 100 DEG C；
Reaction equation is as follows：
。
A kind of described diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method, methyl phenyl vinyl
Silicone oil, viscosity are 30200mPas, and phenyl mass fraction is 55%, and vinyl mass fraction is 3.6%.
A kind of described diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method, metal-oxide is
Fe2O3、 CeO2、 ZnO、 TiO2、 V2O5, above-mentioned oxide using individually one or more, its granularity is 0.1～5
μm scope, the above-mentioned metal-oxide being added in silicone rubber are obtained after silane coupler is processed.
Advantages of the present invention with effect is：
By methyl phenyl vinyl silicone oil in the present invention, diphenyl siloxy cage-type silsesquioxane cross-linking agent, metal-oxide,
PC610 catalyst-initiators, under Pt catalyst actions, cage-type silsesquioxane and the generation addition of silicone rubber medium vinyl are anti-
Should, novel Room Temperature sulphurated siliastic is prepared, the present invention can be used at a temperature of 460 DEG C for a long time, with original silicon rubber
Glue compares thermostability more preferably, easy to use.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
In embodiment, raw material removes specified otherwise, is commercial.
In embodiment, cross-linking agent used is diphenyl siloxy cage-type silsesquioxane
Embodiment 1
Take 100 parts of methyl phenyl vinyl silicone oils, 5 parts of nano tin dioxides, 5 parts of nano-cerium oxides, 0.2 part of PC610,0.5 part of Pt
Platinum catalyst, mechanical agitation mix homogeneously, 100 DEG C of vaccum dewatering 5h.Add 35 parts of diphenyl siloxy cage model sesquialter silicon
Oxygen alkane organosilicon cross-linking agent, the bubble after mix homogeneously in low pressure removing system；Can be completely after heat treatment 4h at 100 DEG C
Solidification.The performance of gained cured glue body is tested according to GB/T 13477.6-2002.
Embodiment 2
Take 100 parts of methyl phenyl vinyl silicone oils, 5 parts of nano tin dioxides, 5 parts of nano-cerium oxides, 0.2 part of PC610,0.5 part of Pt
Platinum catalyst, mechanical agitation mix homogeneously, 100 DEG C of vaccum dewatering 5h.Add 45 parts of diphenyl siloxy cage model sesquialter silicon
Oxygen alkane organosilicon cross-linking agent, the bubble after mix homogeneously in low pressure removing system；Can be completely after heat treatment 4h at 100 DEG C
Solidification.The performance of gained cured glue body is tested according to GB/T 13477.6-2002.
Embodiment 3
Take 100 parts of methyl phenyl vinyl silicone oils, 5 parts of nano tin dioxides, 5 parts of nano-cerium oxides, 0.2 part of PC610,0.5 part of Pt
Platinum catalyst, mechanical agitation mix homogeneously, 100 DEG C of vaccum dewatering 5h.Add 55 parts of diphenyl siloxy cage model sesquialter silicon
Oxygen alkane organosilicon cross-linking agent, the bubble after mix homogeneously in low pressure removing system；Can be completely after heat treatment 4h at 100 DEG C
Solidification.The performance of gained cured glue body is tested according to GB/T 13477.6-2002.
The silicon rubber prepared from data above, present invention pheiiyldimetliyl siloxy cage-type silsesquioxane
Glue, Good Heat-resistance, mechanical property are good.
Claims (3)
1. a kind of diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method, it is characterised in that methods described bag
Include following preparation process：
i）The synthesis of diphenyl siloxy cage-type silsesquioxane；
ii）Methyl phenyl vinyl silicone oil is sequentially added, metal-oxide, PC610 inhibitor, Pt platinum catalysts, machinery are stirred
Mix mix homogeneously, 100 DEG C of vaccum dewatering 5h；Add the diphenyl siloxy cage model sesquialter silicon for being dissolved in hexamethylene of above-mentioned preparation
Oxygen alkane cross-linking agent, the bubble after mix homogeneously in low pressure removing system can be fully cured after heat treatment 4h at 100 DEG C；
Reaction equation is as follows：
。
2. a kind of diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method according to claim 1, its
It is characterised by, methyl phenyl vinyl silicone oil, viscosity is 30200mPas, and phenyl mass fraction is 55%, vinyl quality point
Number is 3.6%.
3. a kind of diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method according to claim 1, its
It is characterised by, metal-oxide is Fe2O3、 CeO2、 ZnO、 TiO2、 V2O5, above-mentioned oxide using individually one or two
More than, its granularity is 0.1～5 μm of scope, and the above-mentioned metal-oxide being added in silicone rubber is all at silane coupler
Obtain after reason.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610916971.XA CN106543732A (en) | 2016-10-21 | 2016-10-21 | A kind of diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610916971.XA CN106543732A (en) | 2016-10-21 | 2016-10-21 | A kind of diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method |
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| CN106543732A true CN106543732A (en) | 2017-03-29 |
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| CN201610916971.XA Withdrawn CN106543732A (en) | 2016-10-21 | 2016-10-21 | A kind of diphenyl siloxy cage-type silsesquioxane heat-resistant silicon rubber preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106633072A (en) * | 2016-12-13 | 2017-05-10 | 沈阳化工大学 | Preparation method of diphenyl siloxyl cage type silsesquioxane heat-resisting silicone rubber |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327273A (en) * | 2014-10-22 | 2015-02-04 | 上海大学 | Organic silicon potting adhesive containing POSS group and preparation method of organic silicon potting adhesive |
-
2016
- 2016-10-21 CN CN201610916971.XA patent/CN106543732A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327273A (en) * | 2014-10-22 | 2015-02-04 | 上海大学 | Organic silicon potting adhesive containing POSS group and preparation method of organic silicon potting adhesive |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106633072A (en) * | 2016-12-13 | 2017-05-10 | 沈阳化工大学 | Preparation method of diphenyl siloxyl cage type silsesquioxane heat-resisting silicone rubber |
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Application publication date: 20170329 |
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